ABSTRACT
Objective: To establish a method for the simultaneous determination of four chromones in Saposhnikoviae Radix by multi-components with single marker ( QAMS) .Methods:An HPLC analysis was used to determine the contents of 4′-O-β-D-glucosyl-5-O-methylvisamminol , cimifugin and sec-O-glucosylhamaudol in Saposhnikoviae Radix.Prim-O-glucosylcimifugin was chosen as the single maker.The contents of 4 chromones in 10 batches of samples were determined by both external standard method and QAMS .The reliability and feasibility of the method were evaluated by the comparison of the quantitative results between the external standard meth -od and QAMS.Results:The relative correction factor (RCF) was perfect.The results calculated by the single marker were consistent with the results from the external standard method .Conclusion:The method with single marker is accurate and feasible to evaluate the quality of Saposhnikoviae Radix.
ABSTRACT
OBJECTIVE:To establish a method for the determination of dendrobine and its metabolites M-250 and M-280 in mice plasma for the first time. METHODS:Mice were given dendrobine 60 mg/kg by intragastric administration,1 h later plasma were collected and treated. Using pseudoephedrine hydrochloride as internal standard and dendrobine reference substance as control, the plasma concentrations of dendrobine and its metabolites M-250 and M-280 were determined by UPLC-MS combined with quantitative analysis of multi-components by single marker. The separation was performed on Hypersil Gold C18 column with 0.1％formic acid-acetonitrile(gradient elution)at the flow rate of 0.3 mL/min. The column temperature was set at 40℃,and sample size was 5 μL. Heatable electrospray ionization (HESI) source, scan/ESI + were applied and operated in positive ion mode with atomization temperature of 300℃,ion transmission tube temperature of 350℃,the sheath gas velocity of 35 arb,the auxiliary air velocity of 15 arb,the spray voltage of 3.5 kV,the collision voltage of 30,40,50 eV. The mass-to-charge ratio of detection range were 100-1500. RESULTS:The endogenous substances of mice plasma had no interference with the content determination of dendrobine and its metabolites M-250 and M-280. The linear range of dendrobine were 9.13-912.94 ng/mL(r=0.9996). The limit of quantitation was 3.04 ng/mL. RSDs of intra-day and inter-day were all less than 7.5％(n=5 or n=3). The accuracy were 96.8％-107.5％(n=5). Matrix effects were 97.1％-106.0％(RSD=1.8％-4.7％,n=5). RSDs of the content of sample at 15℃ for 24 h,at -70 ℃ after three times freeze-thaw,at -70 ℃ for 15 d were lower than 12.8％ (n=3). The content of dendrobine in plasma sample of mice was (41.3 ± 5.7) ng/mL (n=12). The contents of its metabolites M-250 and M-280 were (493.0 ± 73.1) and (41.4 ± 3.0) ng/mL (n=12) with Relative correction factor of 1.0. CONCLUSIONS: The method is sensitive and accurate,and can be used for content determination of dendrobine and its metabolites M-250 and M-280 in mice plasma.
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Objective:To establish a quantitative analysis method for determining the dissolution of Yinxingye dispersible tablets by quantitative analysis of multi-components with single-marker ( QAMS) . Methods:A small glass method was adopted. Hydrochloric acid (0. 1 mol·L-1 ) was used as the dissolution medium, and the stirring speed was at 50 r·min-1 . HPLC-ELSD with gradient elu-tion combined with QAMS was used to simultaneously determine the dissolution of 3 total flavonoids ( artemisinin, quercetin and isorh-amnetin) and 4 total lactones (ginkgo esters and lactones a, b and c) in Yinxingye dispersible tablets. Results:Within a certain line-ar range, the relative correction factors (RCFs) of quercetin and isorhamnetin with the reference of artemisinin was 1. 873 and 0. 324, respectively, and the RCFs of lactones a, b and c with the reference of ginkgo esters was 2. 280, 1. 659 and 1. 429, respectively, and the repeatability was good under the different experimental conditions. There were no significant differences between the calculated val-ues by QAMS and those by the external standard method in 5 batches of Yinxingye dispersible tablets, and the results showed that the RCFs was authentic. The dissolution uniformity of Yinxingye dispersible tablets was good in 0. 1 mol·L-1 hydrochloric acid. Conclu-sion:The method is simple, accurate and reproducible in the dissolution determination of Yinxingye dispersible tablets.
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Objective To establish an HPLC method to measure four flavonoids ( baicalin, wogonoside,baicalein and wogonin) in shenyan siwei granules by quantitative analysis of multi-components with single marker ( QAMS ) . Methods Agilent ZORBAX SB-C18 column(4. 6 mm × 250 mm,5 μm) was used. The mobile phase was composed with methanol and 0. 4% phosphoric acid solutionat at 1. 0 mL·min-1 flow rate with gradient elution. The detection wavelength was 278 nm. Baicalin was used as the internal reference substance. The relative correction factors ( RCF) between the baicalin and the other three flavonoids were established to detect the quantitation of baicalin and calculate the quantitation of the other three constituents. The external standard method was used for quantitating the four constituents, and the method was evaluated by comparing to the quantitative results between external standard method and QAMS method. Results The results of QAMS method had no significant difference with those of external standard method. Conclusion It is feasible and accurate to control the quality of shenyan siwei granules with QAMS.
ABSTRACT
Objective To establish a quality evaluation method for determination of paris saponinⅠ,Ⅱ,Ⅵ,Ⅶ in paridis rhizhma by quantitative analysis of multi-components with single-marker (QAMS).Methods An HPLC method and a Phenomenex Luna C18 column(4.6 mm×250 mm,5 μm)were used.The mobile phase was acetonitrile-water (48:52) at a flow rate of 1.0 mL·min-1.The detection wavelength was 203 nm and column temperature was 25 ℃.Parissaponin Ⅶ was used as the internal reference substance.The relative correlation factors of parissaponinⅠ,Ⅱ,Ⅵ were calculated by standard curve method and QAMS.Results The QAMS method could be used for determination of four saponin components at the same time without significant difference as compared with the results of standard curve method (RSD<2.0%).Conclusion QAMS method is simple and reproducible,which can provide a reference for quality standard revision for paridis rhizhma.